ASTM D3087-17 Standard Test Method for Operating Performance of Anion-Exchange Materials for Strong Acid Removal.pdf

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1、Designation: D3087 17Standard Test Method forOperating Performance of Anion-Exchange Materials forStrong Acid Removal1This standard is issued under the fixed designation D3087; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the ye

2、ar of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the oper-ating capacity of anion-exchange materials when used for t

3、heremoval of hydrochloric and sulfuric acid from water. It isdesigned to simulate operating conditions for strong acidremoval and is intended for use in testing both new and usedmaterials.1.2 The values stated in SI units are to be regarded as thestandard. The inch-pound units given in parentheses a

4、re forinformation only.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior

5、 to use.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBar

6、riers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1067 Test Methods for Acidity or Alkalinity of WaterD1125 Test Methods for Electrical Conductivity and Resis-tivity of WaterD1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2687 Practices for Sampling

7、Particulate Ion-Exchange Ma-terialsD5391 Test Method for Electrical Conductivity and Resis-tivity of a Flowing High Purity Water Sample3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard, refer toTerminology D1129.4. Summary of Test Method4.1 The test method consists o

8、f repeated cycles ofbackwash, base regeneration, rinse, and exhaustion of thesample in the form of a bed in a transparent column. Theexhaustion medium used is an ion-exchange test water.5. Significance and Use5.1 This test method can be used for evaluating performanceof commercially available anion-

9、exchange materials regardlessof the basic strength of the ion exchange groups. Whenprevious operating history is known, a good interpretation ofresin fouling or malfunction can be obtained by comparisonagainst a reference sample of unused ion-exchange materialevaluated in the same way.5.2 While resi

10、stivity has been chosen as the preferredanalytical method for defining the exhaustion end point, withtitration as the alternative, it is understood that observation ofpH during rinse and the service run can yield useful informa-tion. The variations in pH observed with an ion exchangematerial suspect

11、ed of having degraded, can be helpful ininterpretation of performance when compared with similar datafor a reference sample of unused material exhausted in thesame way.6. Apparatus6.1 Test Assembly (see Fig. 1), consisting of the following:6.1.1 Column, transparent, vertically supported, 25.4 62.5-m

12、m (1.0 6 0.1-in.) inside diameter and approximately 1.5m (60 in.) long. The bottom of the column shall be closed andprovided with an outlet of approximately 6-mm (14-in.) insidediameter. Connections shall be provided at the top and bottomfor the admission and removal of the solutions described inSec

13、tion 7. Adequate means for measuring and regulating theflow shall also be provided. The column shall be calibrated in1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.08 on Membranes and IonExchange Materials.Current editio

14、n approved June 1, 2017. Published June 2017. Originallyapproved in 1978. Last previous edition approved in 2009 as D3087 91 (2009).DOI: 10.1520/D3087-17.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS

15、tandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized princi

16、ples on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1such a manner that the volume readings required by the methodcan be made (se

17、e Section 9). All measurements shall be madeat 25 6 5C.6.1.2 Support the sample at least 50 mm (2 in.) above thebottom of the column outlet using quartz, gravel, glass beads orother material from 1.5 to 3.5 mm (116 to18 in.) in diameter,insoluble in the reagents used, and retained on a corrosion-res

18、istant screen. However, other supports may be used at thediscretion of the interested parties.7. Reagents7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analy

19、tical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high puritity to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise

20、 indicated, referencesto water shall be understood to mean reagent water conformingto Specification D1193, Type III.7.3 Acidity Test ReagentsFor reagents used in determiningacidity, refer to Test Methods D1067.7.4 Anion Exchange Test Water C (10 meq/L)Carefullyadd 18.1 mL of sulfuric acid (H2SO4, sp

21、 gr 1.84) and 27.5 mLof hydrochloric acid (HCl, sp gr 1.19) to 500 mL of water anddilute to 1 L. Prepare the test water by adding 1 volume of themixed acid solution to 99 volumes of water. Determine theacidity of the test water in accordance with Test MethodsD1067, titrating to the methyl purple end

22、 point. The acidityshall be 10.0 6 0.5 meq/L (epm).7.5 Base Regenerants:7.5.1 For Weak Base Ion-Exchange Materials:7.5.1.1 Ammonium Hydroxide (40gNH3/L)Dilute 155mL of ammonium hydroxide (NH4OH sp gr 0.90) to 1 L withwater. The solution should be freshly prepared to avoidabsorption of carbon dioxide

23、 (CO2) from the air.7.5.2 For Weak, Intermediate, and Strong Base Ion-Exchange Materials:7.5.2.1 Sodium Hydroxide Solution (40 g/L)Dissolve 40 gof sodium hydroxide (NaOH) in 800 mL of water and dilute to1 L. The solution should be freshly prepared to avoid absorp-tion of carbon dioxide (CO2) from th

24、e air.8. Sampling8.1 For sampling procedures refer to Practices D2687.9. Procedure9.1 Adjust temperature of the water and all solutions to beused in this procedure to 25 6 5C and maintain thistemperature throughout the test.9.2 Fill the column approximately half full of water and addsufficient sampl

25、e to give a bed height of 750 6 75 mm (30 63 in.) above the top of the support. To avoid drying out of theion-exchange material, maintain a layer of liquid at least 20 to30 mm (0.8 to 1.2 in.) deep above the top of the bed at all timesduring the procedure.9.3 Backwash with water for 10 min using a f

26、low rate thatwill maintain a 50 % expansion of the bed. If the supernatantliquid is clear at this point, proceed to 9.4. If the supernatantliquid is cloudy (indicating the presence of light, insoluble,extraneous material), adjust the backwash outlet tube to aheight above the bed equal to 75 % of the

27、 bed height. Continuebackwashing at the same rate until the effluent is clear.9.4 Allow the bed to settle and then drain at a rate ofapproximately 100 mL/min until the water level is 20 to 30 mm(0.8 to 1.2 in.) above the top of the bed. Record the volume, inmillilitres, of ion-exchange material for

28、use in the followingpretreatment. Regenerate the sample with the appropriatedilute sodium hydroxide solution (see Note 1) for 90 min at aflow rate of 0.11 mL/min for each millilitre of ion exchanger inthe column. This corresponds to a regeneration level of 400 g/L(25 lb/ft3) of ion exchange material

29、.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC, www.chemistry.org. For suggestions on thetesting of reagents not listed by the American Chemical Society, see the UnitedStates Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,I

30、nc. (USPC), Rockville, MD, http:/www.usp.org.“Reagent Chemicals,American Chemical Society Specifications,”Am. ChemicalSoc., Washington, DC. For suggestions on the testing of reagents not listed by theAmerican Chemical Society, see “Analar Standards for Laboratory Chemicals,”BDH Ltd., Poole, Dorset,

31、U.K., and the “United States Pharmacopeia.”FIG. 1 Typical Arrangement of Apparatus for Performance Test-ing of Ion-Exchange MaterialsD3087 1729.5 When only a 20 to 30-mm (0.8 to 1.2-in.) layer of liquidremains above the bed, rinse with water using the same flowrate, until a volume equal to the volum

32、e of resin has beendisplaced (one bed volume). Increase the rinse rate to approxi-mately 100 mL/min and continue the rinse until a total of tenbed volumes liquid have been used.9.6 Backwash with water for 10 min using a flow rate thatwill maintain a 50 % expansion of the bed. Allow the bed tosettle

33、and then drain at rate of approximately 100 mL/min untilthe water is 20 to 30 mm (0.8 to 1.2 in.) above the top of thebed. Record the volume in millilitres, of ion-exchange mate-rial. Repeat the foregoing procedure until two successivevolume readings agree within 5 mL. Take the average of thesetwo r

34、eadings as the sample volume used in calculating thecapacity of the ion-exchange material under test.9.7 Exhaust the ion exchange material with the anion-exchange test water C at a flow rate of 0.33 mL/min/mL of ionexchange material as measured in 9.6. Maintain a head ofliquid not less than 50 mm (2

35、 in.) above the top of the bedduring the exhaustion. During the run, test the effluent periodi-cally by one of the methods given in Table 1. Continue the rununtil the designated end point is reached, and record thevolume of test water used.9.8 Repeat the backwash and drain in accordance with 9.6,omi

36、tting the determination of bed volume.9.9 Regenerate the sample with the appropriate NaOHsolution (see Note 1), maintaining a flow rate through the bedof 0.054 mL/min/mL of ion-exchange material based on thesample volume determined in 9.6. Continue the flow for 30min, leaving a 20 to 30-mm (0.8 to 1

37、.2-in.) layer of liquidabove the bed. This corresponds to a regeneration level of 64.1g/L (4 lb/ft3) of ion-exchange material.NOTE 1Alternative regenerant solutions, ammonia and soda ash, maybe used in place of caustic for evaluation of weak base ion-exchangematerial; however, the operating capacity

38、 results based on these regener-ants may be different than the operating capacity results based on causticregeneration.9.10 Rinse the bed with anion-exchange test water C (seeNote 2) at the same rate until one bed volume of liquid hasbeen displaced, then increase the rate to 0.33 mL/min/mL ofion-exc

39、hange material as measured in 9.6. The liquid levelabove the top of the bed should be maintained at 50 mm (2 in.).During the rinse, determine the effluent resistivity at least every15 min, until the resistivity is greater than 20 000 -cm andrecord the volume of rinse water.NOTE 2Test water C is used

40、 for the rinse step to simulate the use ofcation bed effluent for anion bed rinse which is typical in many industrialdemineralizer systems. Alternative rinse solutions, such as water, may beused in the evaluation of other types of systems; however, the operatingcapacity results based on these rinse

41、solutions may be different than thoseusing test water C as required in 9.10.9.11 Exhaust the ion-exchange material by maintaining theflow of test water until the effluent resistivity is less than20 000 -cm. Record the total volume of test water.9.12 Repeat the cycle, beginning with the backwash (see

42、9.8) followed by the regeneration (see 9.9). Continue with therinse (see 9.10) and end with the service run (see 9.11). Repeatuntil each of three successive runs agrees within 6 5 % of theaverage capacity as calculated in accordance with Section 10.10. Calculation10.1 Calculate the operating capacit

43、y, C, in milliequivalentsper millilitre of ion-exchange material as follows:C 5 B 2 A! 3F#/Swhere:A = litres of test water used in rinse (see 9.10),B = total litres of test water used (see 9.11),F = acidity of test water, meq/L, (see 7.4) andS = millilitres of ion-exchange material used (see 9.6).10

44、.2 Calculate the operating capacity, C, in kilograins ofcalcium carbonate per cubic foot, as follows:C 5 C 321.810.3 Calculate the rinse value, R, in litres of rinse water perlitre of bed volume, as follows:R 5 A 31000!/Swhere:A = litres of rinse water (see 9.10), andS = millilitres of ion-exchange

45、material used (see 9.6).10.4 Calculate the rinse value, R , in gallons of rinse waterper cubic foot of bed volume, as follows:R 5 R 37.4811. Report11.1 Report the capacity of test material as the average ofthree successive service runs that agree within 65 % of theaverage.12. Precision and Bias412.1

46、 PrecisionThe Referenced Documents show thatseven laboratories participated in a round robin test of theoperating performance of anion-exchange materials of fourresins using two different regenerants, sodium hydroxide, andammonium hydroxide. Each of the four resin samples wereevaluated by at least t

47、hree different labs and in some cases fourdifferent labs. Each lab evaluated the assigned resin samples atleast once, with three labs doing the assigned samples induplicate, and one lab doing the assigned samples in triplicate.Separate evaluations of two resin samples were made by twopeople in one l

48、ab.4Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D19-1011. ContactASTM CustomerService at serviceastm.org.TABLE 1 Test Methods for Anion-Exchanger EffluentStatus ASTMDesignationRinse EndPointService EndPointPreferred D1125(or

49、D5391)20 000 -cm 20 000 -cmAlternative D1067 0.1 meq/L phenol-phthalein0.1 meq/L methylpurpleD3087 17312.1.1 The precision of the values obtained by this testmethod is dependent upon the magnitude of the observedvalues and can be estimated from the following relationships:12.1.1.1 For rinse values in litre of rinse per litre of resinbed (see 10.3):logSR5 0.0267R 2 0.523where:SR= the absolute value of the standard deviation, andR = rinse value in L of rinse/L of resin bed.12.1.1.2 For capacity values in kilograins per cubic foot asCaCO3(